Refined &#34;sulphate black liquor&#34; talloel and process of making the same



Passed Jan. s, 1935 UNITED STATES SULPHATE BLACK LIQUOR PATENT OFFICE TALLOEL AND PROCESS OF MAKING THE SAME Tonten Halsektrom, New York, N. Y.

No Drawing. Application December 3, 1931,

7 Serial No. s'zasu 13 Claim. (Cl.

refined sulphate black liquor talloel and to a process of producing such refined talloel onan industrial scale.

It is well known in the paper and pulp industry that when black liquor from the sulphate process is evaporated, a scum, known as talloel soap, separates and floats upon the surface of the black liquor. The talloel soap which is skimmed off the evaporated black liquor is ready for treatment. The customary procedure is to add dilute sulphuric acid. Following this addition of acid, the mass separates into two layers, the upper of which contains crude talloel. Many efforts have been made to use crude talloel directly in commerce and industry in a practical and satisfactory manner, and to provide processes of treating the crude talloel to make it available for satisfactory use in commerce and industry; These prior efiorts have been unsuccessful for one reason or another and no completely successful and wholly satisfactory process has been provided for converting crude talloel into an industrially and. commercially useful and satisfactory product.

I have discovered a process of treating sulphate black liquor" .or the talloel soap obtained therefrom .to produce a refined talloel possessing properties which make it valuable and useful as a commercial and industrial product.

It is an object of the invention to provide a simple, economical and practical process for carrying out my discovery on an industrial scale.

It is also within the contemplation of the invention to provide a process which is capable of being operated by relatively unskilled labor and which is capable of producing useful and valuable by-products.

Other objects and advantages will become apparent fromthe following description of a preferred procedure for carrying the present invention into practice.

Black liquor produced in the sulfate process of producing pulp and paper is used as the raw material and is termed herein sulfate black liquor" for convenience. The black liquor is evaporated until! the talloel soap separates. The exact specific gravity to which the black liquor must be evaporated before the talloel soap separates depends upon the alkalinity and viscosity of the black liquor as one skilled in the art readily understands. When the black liquor has been evaporated as aforesaid, crude talloel soap separates and floats on the surfaceof the evaporated liquor. By skimming off the fioating'scum, crude talloel soap may be obtained.

The crude talloel soap is treated with a suitable acid or acid substance, such as sulphuric acid or acid sodium sulphate, to liberate crude talloel. In practice dilute sulphuric acid having a concentration of about 10-20% or an eight normal solution of acid sodium sulphate has been found to give satisfactory results. After the acid has I have found that the crude talloeLwhich is not very useful, can be converted into a highly useful refined product by removing certain constituents. These constituents can be removed satisfactorily by permitting the talloel to stand for a period of time, say about 2 days to about 10 days or so at atmospheric temperatures. Among the constituents, which are practically completely removed, may be mentioned ligneous matters and higher saturated fatty acids. In addition the refined product contains reduced amounts of oxidized colophonic acids and colophonic acids (classified according to Aschans system) and of non-saponifiable matter than the crude talloel. In practice, the foregoing constituents separate out from the talloelon standing and may be removed by filtering, decanting, or the like. The filtrate is refined talloel which is relatively stable and which is very useful commercially and industrially. Among the important uses, I have discovered for refined talloel, soap making and fiotation of certain ores of the alkaline earth metals may be mentioned. This latter discovery is described and claimed in a copending application, Serial No. 578,842 and filed December 3rd, 1931.

In some instances, the refining operation may be carried still further. For instance, by refrigerating the talloel at a temperature within a range of about 25 C. to about minus 10 0.. say about 0' C. and maintaining it at the refrigerated temperature for a period of say a week to ten days or so, with'or without aeration, it is possible to remove further constituents from the talloel. The solids which have separated from the liquid may be removed by filtering or the like. By this operation, odorous products, colophonic acids, oxidized colophonic acids, etc. are removed. The filtrate is a super-refined tallod and is useful and available for additional purposes. Thus, it may be used for making'laundry and other soaps.

In the event it is desired to de-colorize my rcfined or super-refined talloel, it may be accomplished in any appropriate or well known manner. For instance, the refined or super-refined talloel may be decolorized with carbon, fuller's earth, sulphur dioxide or the like in accordance with well known procedures.

It has also been found that the solids separated from the liquid talloel can be melted together to form a product which can be used as a substitute for rosin. The solids may be used separately for the aforesaid purpose, if it is desired. It will thus be observed that the by-products are useful and valuable instead of being useless.

It will be observed that the present invention provides a process of producing a purified and refined talloel which has a fairly low viscosity, which can be pumped like a liquid and which can be shipped in barrels and tank cars as an article of commerce.

It will be noted that the present invention provides a purified and refined talloel which has the following properites: My refined talloel is substantially devoid of ligneous matters and/or higher saturated fatty acids of sulphate black liquor, and contains reduced amounts of colophonic acids, oxidized colophonic acids and/or non-saponifiable matter. The acid number varies but is approximately 190 to about 200. In the same way, the iodine number varies but is approximately 200 to about 210 according to the Hanus method. The specific gravity at about 20 C. is more than about 0.89 and less than about 1.00. The viscosity is fairly low; the color varies but is usually reddish brown; and the odor sanewhat resembles that of a mixture of pine oil and rosin. Moreover, the refined talloel is relatively stable as an article of commerce and practically no solid matter separates upon standing for a reasonable length of time, say about two weeks to about ten weeks;

It will be further noted that the present invention provides a purified and super-refined talloel which has the following properties: The acid number varies but is approximately 180 to about 190. Similarly, the iodine number varies but is approximately to about according to the Hanus method. The specific gravity varies from about 0.90 to about 0.97 at about 20 C. The super-refined talloel has a fairly pleasant odor resembling that of a mixture of pine oil and rosin, has a reddish yellow to yellow color and is sub-' stantially devoid of ligneous matter, and/or higher saturated fatty acids of sulphate black liquor. The viscosity is less than that of my refined talloel. Practically no solid matter separates upon standing for a reasonable length of time, such as two weeks to ten weeks. and the superrefined talloel is a relatively stable article of comemployed. Other modes of separating my refined or super-refined talloel from the imdersirable solid constituents mentioned herelnabove may be employed, such as vacuum distillation with or without the use of steam. Furthermore, filter aids, such as kieselgur, sil-o-cel, diatomaceous earth, and the like, may be employed to facilitate filtration or separation of the undesired solid constituents.

It is to be noted that the raw material or crude talloel soap is obtained from black liquor of the sulphate process of paper or pulp making. This process is well known to chemists and is not to be confused with the sulphite process or other processes. The liquor obtained from these processes would not yield my refined talloel or super-refined talloel.

I claim:-

1. Refined, non-distilled, liquid talloel substantially devoid of solid constituents and of ligneous matters of sulphate black liquor and containing substantial amounts of resin acids.

2. Refined, non-distilled, liquid talloel substantially devoid of solid constituents and of higher saturated fatty acids of sulphate black liquor and containing substantial amounts of resin acids.

3. Refined, non-distilled, liquid talloel substantially devoid of solid constituents and of ligneous matters and of higher saturated fatty acids of sulphate black liquor, said refined liquid talloel containing substantial amounts of resin acids.

4. Refined, non-distilled, liquid talloel substantially devoid of solid constituents and containing reduced amounts of oxidised eolophonic acids and of non-saponifiable matter and containing substantial amounts of resin acids.

5. Refined, non-distilled, liquid talloel substantially devoid of solid constituents and substantial- Lv devoid of ligneous matters and of higher saturated fatty acids of sulphate black liquor and containing reduced amounts of oxidised colophonic acids and of non-saponifiable matter, said refined liquid talloel containing substantial amounts of resin acids.

6. Refined liquid talloel having an acid number of about to about 200, an iodine number of about 200 toabout 210 according to Hsnus method and a specific gravity of more than 0.89 to less than 1.00 at about 20' C.

7. The processofproducingrefinedtalloel from sulphate black liquor which comprises evaporating black liquor until talloel soap separates, separating talloel soap from the surface of the evaporated black liquor, treating said talloel soap with an acid substance to form a liquid mass, permitting said mass to separate into two layers, separating the upper layer containing crude talloel from the lower layer, permitting said crude talloel to stand foraboutfl daystoabout lodaystoefiectseparation of'detrimental solid constituents including ligneous matters and higher saturated fatty acids, and separating said solid constituents from the liquid whereby a refined talloel is produced.

8. The process of producing refined talloel from crude talloel soap of sulphate black liquor which comprisesreactingcrudetalloelsoapwithan a'queous acid solution to form a liquid mass, permittingsaidmasstoseparateintotwolsyersby standing, separating the upper layer containing msdetalloelfromthelowerlayer.remov'ingcnly detrimental solid constituents including ligneous matter and higher saturated fatty acids from said crude talloel, and separating said solid constitumtsfromtheliquidwherebyarefincdiiquid talloel b produced.

'9. The process of producing refined talloel from crude talloel soap of sulphate black liquor which comprises treating crude talloel soap with an acid sulphate solution to form a liquid mass, permitting said mass to separate into two layers, separating the upper layer containing crude talloel from the lower layer, permitting said crude tal- -loel to stand for a period of about 2 days to about 10 days to effect separation of detrimental solid constituents including ligneous matter and higher saturated fatty acids, and separating said solidconstituents from the liquid whereby a refined talloel is produced.

10. The process of producing refined talloel from sulphate black liquor which comprises evapcrating black liquor until talloel soap separates, separating talloel soap from the surface of the evaporated black liquor, treating said talloel soap with an acid substance to form a liquid mass, permitting said mass to separate into two layers, separating the upper layer containing crude talloel from the lower layer, permitting said crude talloel to stand for about 2 days to about 10 days to effect separation of detrimental solid constituents including ligneous matters and higher saturated fatty acids, and separating said solid constituents from the liquid whereby a refined talloel is produced, and maintaining said refined talloel at a temperature within a range of about minus 10 C. to about 25 C. to efiect a further separation of detrimental solid constituents.

11. The process of producing refined talloel from crude talloel soap of sulphate black liquor which comprises reacting crude talloel soap with an acid solution to form a liquid mass, permitting said mass to separate into two layers, separating the upper layer containing crude talloel from the lower layer, treating said crude talloel to effect a separation of detrimental solid constituents including ligneous matter and higher saturated fatty acids. and separating said solid constituents from the liquid whereby a refined talloelis produced, and maintaining said refined talloel at a temperature within a range of about minus 10' C. to about 25 C. to eifect a further separation of detrimental solid constituents.

'12. The process of producing refined talloel from crude talloel soap of sulphate black liquor which comprises reacting crude talloel soap with an aqueous acid solution to form a liquid mass, permitting said mass to separate into two layers by standing, separating the upper layer containing crude talloel from the lower layer, removing only detrimental solid constituents including solid ligneous matter, solid acids and the like, and

TORBTEN HASSELSTROM. 

